CN107151015A - A kind of preparation method of luffa nitrogen-doped carbon nano material - Google Patents
A kind of preparation method of luffa nitrogen-doped carbon nano material Download PDFInfo
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- CN107151015A CN107151015A CN201710500847.XA CN201710500847A CN107151015A CN 107151015 A CN107151015 A CN 107151015A CN 201710500847 A CN201710500847 A CN 201710500847A CN 107151015 A CN107151015 A CN 107151015A
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- luffa
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of preparation method of luffa nitrogen-doped carbon nano material.Comprise the following steps that：(1) picked after luffa is gathered, go to plant, removal of impurities, dry, pulverize after wash clean, (2) take the powder of luffa in tube furnace, are passed through the nitrogen by urea liquid, nitrogen carries urea liquid and the powder of luffa is calcined together, obtains pre-product；(3) powder adds stir process in KOH solution after being calcined, and obtains intermediate product, (4) intermediate product is calcined at high temperature obtains product a, (5) a is handled with hydrochloric acid solution, wash again to neutrality, drying, obtain luffa nitrogen-doped carbon nano material.The beneficial effects of the present invention are：It is raw material using luffa, urea is increase nitrogen source, prepares the nano material of nitrogen-doped carbon, it is proposed that a kind of preparation method of new biomass carbon material, preparation technology is simple, abundant raw material, can quantify production, belongs to environmentally friendly material.
Description
Technical field
Present invention relates particularly to technical field of nano material, more particularly to a kind of luffa nitrogen-doped carbon nano material
Preparation method.
Background technology
Luffa is the vascular bundle of the ripening fruits of cucurbitaceous plant sponge gourd, also known as day trailing plants muscle, chalina, Hypericum perforatum L etc.,
Former plant Guangdong sponge gourd also known as：Patola, medically has clearing and activating the channels and collaterals, effect of removing toxicity for detumescence.Luffa is by vascular bundle
It is crisscross to form, mostly Long Circle, different in size, rough surface, it is yellow in band it is white, very gently, high resilience, gas is micro-, taste
It is light.There are the particular matters such as abundant wood glue citrulling among sponge gourd, vitamin of skin aging etc. is also prevented containing skin whitening
Composition, can protect skin, make skin pure white, so Sucus Luffae has " beauty's water " good reputation.Luffa is a kind of new ring
Environment-friendly materials are protected, luffa living resources are developed and utilized and play unique functional characteristic, is hopeful to become nitrogen and mixes
The desirable feedstock of miscellaneous carbon nanomaterial.
Carbon material is a kind of highly stable chemical substance, at room temperature almost into chemical inertness, the unique property of carbon material
Matter and form cause the interest of numerous researchers, it be in the periodic table of elements it is unique have it is different from zero dimension to three-dimensional homoatomic
The element of body.The factors such as dimension, size and the pattern of carbon material all have a significant impact to the performance of material, and pass through nitrogen
Source is introduced into the application that can improve it in ultracapacitor etc., and the carbon material of N doping is the important set of carbon nanometer technology
Into part, there is important application in terms of electrochemistry and catalysis.
There are many deficiencies in existing nitrogen-doped carbon nano material preparation technology, such as the environment synthesized is not environmentally friendly enough, closes
Into process it is excessively cumbersome, the requirement to consersion unit is higher, production cost height etc..
The content of the invention
The defect and deficiency existed for existing nitrogen-doped carbon material, the present invention proposes a kind of luffa nitrogen-doped carbon and received
The preparation method of rice material, the preparation method proposes a kind of preparation method of new biomass nitrogen-doped carbon nano material,
The abundant raw material of this method, preparation technology is relatively simple, and production cost is low, can realize quantization production.
Technical solution of the present invention is specifically described as follows.
A kind of preparation method of luffa nitrogen-doped carbon nano material, is comprised the following steps that：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried, pulverize after wash clean；
(2) take the powder of luffa in tube furnace, be passed through the nitrogen by urea liquid, nitrogen carry urea liquid and
The powder of luffa is calcined to black at a temperature of 200 DEG C -800 DEG C together, obtains pre-product；
(3) pre-product is added into stir process in KOH solution, processing time is 4h-48h and then carries out drying and processing, is obtained
To intermediate product；
(4) intermediate product is calcined 1~5h at a temperature of 600-900 DEG C, product after being calcined, after baking be for
Pore-creating activation is carried out to the carbon material that KOH is etched；
(5) by product hydrochloric acid impregnation process after the roasting of step (4), dipping filters after terminating, washs drying and processing again,
Obtain luffa nitrogen-doped carbon nano material.
In the present invention, in step (1), drying time is 24h48h, and the luffa vegetable sponge of 50-100 mesh is made in grinding.
In the present invention, in step (2), urea concentration is 1-6mol/L, and nitrogen enters tube furnace by urea liquid, is led to
Enter nitrogen flow rate for 20ml/min-100ml/min, roasting time is 1h-5h.It is preferred that, sintering temperature is 200~400 DEG C,
Roasting time is 3h-5h.
In the present invention, in step (3), the mass ratio of KOH and pre-product is 1:1-1：3, the concentration of KOH solution is 1-
4mol/L。
In the present invention, in step (5), the concentration of hydrochloric acid is 1~3mol/L, and the HCl treatment time is 12h-36h.
Compared with prior art, the beneficial effects of the present invention are：
1st, the present invention not only contributes to improve the utilization rate of luffa, turned waste into wealth, also have directly using luffa as raw material
Beneficial to environmental protection, the recycling of abandoned biomass is realized, effectively the production cost of reduction nitrogen-doped carbon material, improve sponge gourd
The ecology of network, social and economic benefit, meet the requirement that country greatly develops abandoned biomass.
2nd, extensively, environmental protection, safety coefficient is higher, can realize biodegradation for luffa raw material sources of the invention,
Biocompatibility preferably, will not be caused environment pollution.
3rd, the present invention is prepared nitrogen-doped carbon nano material using luffa there is provided a kind of new biomass N doping
The preparation method of carbon material, preparation technology is simple, pollution-free, can quantify production.
Brief description of the drawings
Fig. 1 is the SEM figures of the luffa nitrogen-doped carbon nano material of embodiment 1.
Fig. 2 is the SEM figures of the luffa nitrogen-doped carbon nano material of embodiment 2.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The other embodiment obtained, belongs to the scope of the present invention.
Embodiment 1
A kind of preparation method of luffa nitrogen-doped carbon nano material, specifically includes following steps：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried after wash clean, drying temperature is 100 DEG C, drying time
Powder is then ground to for 36h, the luffa vegetable sponge of 50 mesh is made；
(2) take the powder of a certain amount of luffa in tube furnace, gas enters tube furnace, urea concentration by urea liquid
For 3M, gas flow rate is passed through for 30ml/min, is calcined at a temperature of 700 DEG C to black, and roasting time is that 1h obtains pre- production
Thing；
(3) mass ratio of preparation KOH solution, KOH and pre-product is 1:1, KOH solution concentration is 2M, by the powder after roasting
End adds stir process in solution, and processing time is 4h and then carries out drying and processing, obtains intermediate product；
(4) intermediate product for obtaining step (3) is calcined under 600 DEG C of high temperature, and roasting time is that 1h obtains product a；
(5) a certain amount of hydrochloric acid solution processing a is prepared, the HCl treatment time is 24h, is finally washed with deionized water and ethanol
Wash to neutrality, drying and processing, drying temperature is 60 DEG C, just obtains luffa nitrogen-doped carbon nano material.Can be clear from Fig. 1
Find out clearly, the luffa nitrogen-doped carbon nano material prepared by said process has an obvious layer structure, layer and layer it
Between form many and big hole again, more complete appearance structure is maintained, it can also be seen that other fragment, it may be possible to due to
Caving in for structure is caused during roasting and etching.
Embodiment 2
A kind of preparation method of luffa nitrogen-doped carbon nano material, specifically includes following steps：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried after wash clean, drying temperature is 100 DEG C, drying time
Powder is then ground to for 36h, the luffa vegetable sponge of 50 mesh is made；
(2) take the powder of a certain amount of luffa in tube furnace, gas enters tube furnace, urea concentration by urea liquid
For 3M, gas flow rate is passed through for 30ml/min, and 600 DEG C of roastings to black, roasting time is that 1h obtains pre-product；
(3) mass ratio of preparation KOH solution, KOH and pre-product is 1:2, KOH solution concentration is 2M, by the powder after roasting
End adds stir process in solution, and processing time is 4h and then carries out drying and processing, obtains intermediate product；
(4) intermediate product for obtaining step (3) is calcined under 600 DEG C of high temperature, and roasting time is that 1h obtains product a；
(5) a certain amount of hydrochloric acid solution processing a is prepared, the HCl treatment time is 24h, is finally washed with deionized water and ethanol
Wash to neutrality, drying and processing, drying temperature is 60 DEG C, just obtains luffa nitrogen-doped carbon nano material.Can be clear from Fig. 2
Find out clearly, the luffa nitrogen-doped carbon nano material prepared by said process has an obvious layer structure, layer and layer it
Between form many and big hole again, more complete appearance structure is maintained, it can also be seen that other fragment, it may be possible to due to
Caving in for structure is caused during roasting and etching.
Embodiment 3
A kind of preparation method of luffa nitrogen-doped carbon nano material, specifically includes following steps：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried after wash clean, drying temperature is 100 DEG C, drying time
Powder is then ground to for 36h, the luffa vegetable sponge of 50 mesh is made；
(2) take the powder of a certain amount of luffa to be calcined in tube furnace to black for 800 DEG C, pass the gas through urea liquid,
Urea concentration is 4M, is passed through gas flow rate for 60ml/min, and roasting time is that 1h obtains pre-product；
(3) mass ratio of preparation KOH solution, KOH and pre-product is 1:2, KOH solution concentration is 2M, by the powder after roasting
End adds stir process in solution, and processing time is 4h and then carries out drying and processing, obtains intermediate product；
(4) intermediate product for obtaining step (3) is calcined under 700 DEG C of high temperature, and roasting time is that 1h obtains product a；
(5) a certain amount of hydrochloric acid solution processing a is prepared, the HCl treatment time is 24h, is finally washed with deionized water and ethanol
Wash to neutrality, drying and processing, drying temperature is 60 DEG C, just obtains luffa nitrogen-doped carbon nano material.
Embodiment 4
A kind of preparation method of luffa nitrogen-doped carbon nano material, specifically includes following steps：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried after wash clean, drying temperature is 100 DEG C, drying time
Powder is then ground to for 36h, the luffa vegetable sponge of 50 mesh is made；
(2) take the powder of a certain amount of luffa to be calcined in tube furnace to black for 900 DEG C, pass the gas through urea liquid,
Urea concentration is 4M, is passed through gas flow rate for 60ml/min, and roasting time is that 1h obtains pre-product；
(3) mass ratio of preparation KOH solution, KOH and pre-product is 1:2, KOH solution concentration is 2M, by the powder after roasting
End adds stir process in solution, and processing time is 4h and then carries out drying and processing, obtains intermediate product；
(4) intermediate product for obtaining step (3) is calcined under 800 DEG C of high temperature, and roasting time is that 2h obtains product a；
(5) a certain amount of hydrochloric acid solution processing a is prepared, the HCl treatment time is 24h, is finally washed with deionized water and ethanol
Wash to neutrality, drying and processing, drying temperature is 60 DEG C, just obtains luffa nitrogen-doped carbon nano material.
Embodiment 5
A kind of preparation method of luffa nitrogen-doped carbon nano material, specifically includes following steps：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried after wash clean, drying temperature is 100 DEG C, drying time
Powder is then ground to for 36h, the luffa vegetable sponge of 50 mesh is made；
(2) take the powder of a certain amount of luffa to be calcined in tube furnace to black for 900 DEG C, pass the gas through urea liquid,
Urea concentration is 5M, is passed through gas flow rate for 100ml/min, and roasting time is that 2h obtains pre-product；
(3) mass ratio of preparation KOH solution, KOH and pre-product is 1:2, KOH solution concentration is 2M, by the powder after roasting
End adds stir process in solution, and processing time is 4h and then carries out drying and processing, obtains intermediate product；
(4) intermediate product for obtaining step (3) is calcined under 800 DEG C of high temperature, and roasting time is that 3h obtains product a；
(5) a certain amount of hydrochloric acid solution processing a is prepared, the HCl treatment time is 24h, is finally washed with deionized water and ethanol
Wash to neutrality, drying and processing, drying temperature is 60 DEG C, just obtains luffa nitrogen-doped carbon nano material.
The above is only the basic explanation under present inventive concept, and according to technical scheme done it is any etc.
Effect conversion, all should belong to protection scope of the present invention.
Claims (6)
1. a kind of preparation method of luffa nitrogen-doped carbon nano material, it is characterised in that comprise the following steps that：
(1) picked after luffa is gathered, go to plant, removal of impurities, dried, pulverize after wash clean；
(2) powder of luffa is taken in tube furnace, the nitrogen by urea liquid is passed through, and nitrogen carries urea liquid and sponge gourd
The powder of network is calcined to black at a temperature of 200 DEG C -800 DEG C together, obtains pre-product；
(3) pre-product is added into stir process in KOH solution, processing time is 4h-48h, drying and processing is then carried out, in obtaining
Between product；
(4) intermediate product is calcined 1~5h at a temperature of 600-900 DEG C, product after being calcined；
(5) by product hydrochloric acid impregnation process after the roasting of step (4), dipping filters after terminating, washs drying and processing again, obtains
Luffa nitrogen-doped carbon nano material.
2. the preparation method of luffa nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (1)
In, drying time is 24h48h, and the luffa vegetable sponge of 50-100 mesh is made in grinding.
3. the preparation method of luffa nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (2)
In, urea concentration is 1-6mol/L, is passed through gas flow rate for 20ml/min-100ml/min, roasting time is 1h-5h.
4. the preparation method of luffa nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (2)
In, sintering temperature is 200~400 DEG C, and roasting time is 3h-5h.
5. the preparation method of luffa nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (3)
In, the mass ratio of KOH and pre-product is 1:1-1：3, the concentration of KOH solution is 1-4mol/L.
6. the preparation method of luffa nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (5)
In, the concentration of hydrochloric acid is 1~3mol/L, and the hydrochloric acid impregnation process time is 12h-36h.
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| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN105752969A (en) * | 2016-02-29 | 2016-07-13 | 武汉理工大学 | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
-
2017
- 2017-06-27 CN CN201710500847.XA patent/CN107151015A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121512A (en) * | 2007-04-29 | 2008-02-13 | 武汉理工大学 | Preparation method for plant active carbon fibre column |
| CN103420369A (en) * | 2012-05-22 | 2013-12-04 | 中国科学院城市环境研究所 | Preparation method of active carbon by adopting zinc chloride activated loofah sponge |
| CN103449433A (en) * | 2012-06-01 | 2013-12-18 | 中国科学院城市环境研究所 | Method for preparing novel active carbon by using potassium hydroxide activated vegetable luffa sponge |
| CN103920460A (en) * | 2014-04-11 | 2014-07-16 | 武汉理工大学 | Method for preparing high-performance biomass activated carbon fibers |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN105752969A (en) * | 2016-02-29 | 2016-07-13 | 武汉理工大学 | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
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